CN108185424B - Carotenoid microparticle preparation and process for producing the same - Google Patents

Carotenoid microparticle preparation and process for producing the same Download PDF

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CN108185424B
CN108185424B CN201711456450.1A CN201711456450A CN108185424B CN 108185424 B CN108185424 B CN 108185424B CN 201711456450 A CN201711456450 A CN 201711456450A CN 108185424 B CN108185424 B CN 108185424B
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carotenoid
preparation
wall material
starch
emulsion
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CN108185424A (en
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李倩
陈剑彬
陈碧聪
吴文忠
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Innobio Corp ltd
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/20—Agglomerating; Granulating; Tabletting
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/045—Hydroxy compounds, e.g. alcohols; Salts thereof, e.g. alcoholates
    • A61K31/07—Retinol compounds, e.g. vitamin A
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005—Wall or coating material
    • A61K9/5021—Organic macromolecular compounds
    • A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

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Abstract

The preparation is a particle preparation prepared by emulsifying and granulating a raw material mixture containing carotenoid and a gelation wall material; the method is characterized in that the gelatinized wall material is obtained by gelatinizing a wall material mixture of starch and carbohydrate in a mass ratio of 1-5: 1. The invention overcomes the inherent defects of carotenoid raw materials in application, and solves the problems of low bioavailability, poor water solubility and the like; and the mechanical strength and stability of the carotenoid particle preparation are greatly improved by selecting and combining the gelation wall material and the deoxidizer, and the carotenoid particle preparation can be applied to the fields of preparing foods, medicines, health-care products and functional foods.

Description

Carotenoid microparticle preparation and process for producing the same
Technical Field
The invention relates to a carotenoid preparation and a preparation method thereof.
Background
Carotenoids (carotenoids) are yellow, orange-red or red polyenes, generally composed of 8 isoprenoid units, of the formula C40H56. It is known that carotenoids have beneficial effects on health, such as it is pro-vitamin a, and can prevent nyctalopia, resist oxidation, prevent cancer, and have strong coloring power. Carotenoids are physiological antioxidants that block lipid peroxidation and thus protect the follicle and uterine steroidogenic cells from oxidation. However, carotenoids are insoluble in water, have low solubility in fats and oils, and are unstable to light, oxygen, and heat. This limited solubility and high sensitivity to oxygen greatly limits carotenoidsThe use of (1).
Many methods have been disclosed to improve the rate of staining and to increase the rate of absorption or bioavailability, and microencapsulation is one of the most effective and concise. Microcapsules are a technology for encapsulating and sealing solid, liquid or gaseous substances in a microcapsule to form a solid particle product. Thus, the embedded components can be protected and isolated from the outside environment, the original color, flavor, performance and biological activity can be maintained to the maximum extent, and the damage and loss of nutrient substances can be prevented. The application field of the Beadlets particles prepared by the microcapsule technology can be expanded. The carotenoid particle preparation product has high hardness and is mainly suitable for producing tablets and hard capsule products. Meanwhile, the carotenoid preparation can also improve the stability of sensitive carotenoid crystals or ointment by utilizing the protection of protective colloid.
However, even if the carotenoid is microencapsulated, the carotenoid content is reduced by the influence of light, oxygen, heat and acid during the storage and application of the product. The quality of the microencapsulation is determined by the quality of the wall material and the preparation method, and the optimization exploration of the carotenoid microencapsulation wall material and the preparation method by the technical personnel in the field is never stopped. How to improve the embedding property of the wall material, optimize the preparation process, remove the influence of oxygen in the system on the carotenoid during preparation, and obtain the carotenoid particle preparation with high hardness and good stability is the key point of the research of the invention.
Disclosure of Invention
The invention aims at providing a novel carotenoid particle preparation, which is prepared by granulating a raw material mixture containing carotenoid and a gelation wall material after emulsification treatment; the gelatinized wall material is obtained by gelatinizing a wall material mixture of starch and carbohydrate in a mass ratio of 1-5: 1.
Further, the present invention is directed to a method for preparing the above carotenoid microparticle preparation, comprising the steps of
a) Preparing the raw material mixture into emulsion with the particle size of 0.5-1 mu m;
b) granulating to obtain carotenoid microparticle preparation.
The invention overcomes the inherent defects of carotenoid raw materials in application by using the microencapsulation technology, and solves the problems of low bioavailability, poor water solubility and the like; and the mechanical strength and stability of the carotenoid particle preparation are greatly improved by selecting and combining the gelation wall material and the deoxidizer. Based on the above, the invention further provides the application of the carotenoid microparticle preparation in the preparation of foods, medicines, health-care products and functional foods.
Detailed Description
The invention provides a carotenoid microparticle preparation and a preparation method thereof.
The carotenoid microparticle preparation is prepared by emulsifying a raw material mixture containing carotenoid and a gelation wall material and granulating; wherein the gelatinized wall material is obtained by gelatinizing a wall material mixture of starch and carbohydrate in a mass ratio of 1-5: 1.
The selection and proportion of starch and carbohydrate in the mentioned wall material mixture are important technical characteristics for realizing the effect of the invention. In particular embodiments, the starch is a modified starch; sodium starch octenyl succinate is preferred. The carbohydrate is selected from the group consisting of saccharides having 10 or less monosaccharides linked by glycosidic linkages to form a straight chain or branched chain, and examples thereof include, but are not limited to, sucrose, glucose syrup, fructose, maltose, lactose, xylose, isomaltooligosaccharide, fructooligosaccharide, corn syrup solids, stachyose, galactooligosaccharide, and mixtures thereof. Among them, glucose syrup having a solid content of 40 to 90% or a mixture thereof in any ratio is particularly preferable. In terms of amount determination, the mass ratio of starch to carbohydrate is 1-5:1, preferably 1-4:1, most preferably 3: 1. The references in this specification and mixtures thereof, unless otherwise stated, refer to mixtures of any 2 or more than 2 of the foregoing components, in any proportions.
Another important feature of the present invention is the gelation treatment of the wall material mixture. The gelation treatment comprises preparing wall material mixture into 45-70% solid content water solution, stirring at 60 deg.C for dispersing and dissolving for 30min, and stirring at 70-90 deg.C for 15-100 min. In a preferred embodiment, the stirring is carried out at 80-90 ℃ for 15-60min, preferably 15-30 min. Under the conditions, the gelatinized wall material prepared by the starch fluidized bed process has the particle size of 1-2mm, the bulk density of 0.75-0.8g/ml, the particle hardness of over 100N and the gel freezing strength of 70-100 bloom.
The amount of the gelling wall material is 30-65%, preferably 40-60%, more preferably 45-55% of the final product mass, calculated on the basis of the final product mass of the carotenoid microparticle formulation.
In another embodiment of the present invention, the raw material mixture further comprises an antioxidant selected from the group consisting of tocopherol, ascorbic acid fatty acid ester, butylated hydroxytoluene, and a mixture of a carotenoid and a gelling wall material
(BHT), Butyl Hydroxyanisole (BHA), propyl gallic acid, tert-butyl hydroxyquinoline, or mixtures thereof; the dosage of the antioxidant is 0.1-10% of the mass of the carotenoid microparticle preparation. Preferably 1% to 5%.
The emulsion prepared from the raw material mixture contains oxygen, the oxygen in the emulsion has great influence on the preparation process of particles and the obtained product in the microencapsulation process, common methods for deoxidizing the emulsion through vacuumizing, introducing nitrogen and the like can only remove bubbles in the system, and the dissolved oxygen in the emulsion cannot be removed through the method. In order to remove dissolved oxygen, according to another embodiment of the present invention, a deoxidizer is added to the emulsion obtained after the raw material mixture is emulsified to remove oxygen in the emulsion. Many of the deoxidizing agents described in the prior art are useful for deoxidizing emulsions. In the embodiment of the present invention, ascorbic acid and/or sodium ascorbate are selected to obtain the residual oxygen amount (residual oxygen amount) of the emulsion
Is 0.1-0.3 mg/L. In addition to the effective removal of oxygen from the emulsion, we have found in the experiments that the use of ascorbic acid and/or sodium ascorbate as a deoxidizer also increases the stability of the product, which is not only related to low oxygen content in the solution, as demonstrated by the data from the comparative experiments. This effect is particularly pronounced when a combination of ascorbic acid and sodium ascorbate is used as a deoxidizer. In the ascorbic acid and sodium ascorbate composition, ascorbic acid and sodium ascorbate are mixed in a mass ratio of 1:1-5, preferably 1: 1-4.
In the technical scheme of the invention, the dosage of the deoxidizer is 1-10%, preferably 2-7%, and more preferably 3-6% of the final product mass of the carotenoid microparticle preparation. The pH value of the deoxidizer used in the emulsion is 3-6, preferably 3.5-4.5. The pH of the emulsion is adjusted by means of a 0.1M sodium hydroxide solution and anhydrous citric acid.
In the carotenoid microparticle preparation, the carotenoid is selected from lutein, zeaxanthin, lycopene, alpha-carotene, beta-carotene, canthaxanthin, lutein ester, astaxanthin or a mixture thereof.
In another aspect, the method for preparing the carotenoid microparticle formulation of the present invention comprises the steps of:
a) preparing the raw material mixture into emulsion with the particle size of 0.5-1 mu m;
b) granulating to obtain carotenoid microparticle preparation.
When applied to the preparation of a preferred mode of carotenoid microparticle formulation, i.e., a product containing a deoxidizer, the preparation method should adaptively include the relevant steps, i.e., the method includes the steps of:
a) preparing the raw material mixture into emulsion with the particle size of 0.5-1 mu m;
b) adding a deoxidizing agent to remove oxygen in the emulsion;
c) granulating to obtain carotenoid microparticle preparation.
In any of the above embodiments of the preparation method, in the step a), the method for preparing the raw material mixture into the emulsion may be: the raw material mixture is instantly melted for 5s at 120 ℃, and then is homogenized twice under high pressure of 45 +/-5 Mpa or dispersed for 30min at high speed by using a colloid mill to prepare the emulsion with the grain diameter of 0.5-1 mu m.
In any of the above embodiments of the preparation method, in the step c), i.e. the granulation step, the granulation method may be wet granulation, dry granulation, spray drying, starch fluidized bed granulation, spray condensation and other granulation methods known in the industry.
The bulk density of the carotenoid particle preparation is 0.8g/ml, and the content of the product is stable for 6 months under the conditions of 40 ℃ and 75% of Relative Humidity (RH); the tablets obtained after compression were stable for 6 months at 40 ℃ under Relative Humidity (RH) of 75%. It can be used as a raw material for further processing into dietary supplement in the form of tablet, capsule, or food and functional food in the form of solid beverage, energy bar or candy.
The following non-limiting examples further illustrate the invention but should not be construed as limiting the invention in any way, as the following methods are employed in the present application to measure and evaluate the product, unless otherwise specified.
The hardness of the gelation wall material is measured by an echolocation automatic particle strength tester FT801, and the gel freezing force of the gelation wall material is measured by a Asahi JS-II freezing force tester.
The residual oxygen content is measured by a Merterler model S4 dissolved oxygen meter.
In the invention, the microencapsulation efficiency is expressed by adopting the surface pigment content, and the higher the surface pigment content is, the lower the microencapsulation efficiency is, the more the non-embedded carotenoid is, and the lower the stability is. The method for measuring the surface pigment content comprises the following steps: adding 5g of microcapsule product to be detected into an eggplant-shaped bottle, adding 20ml of petroleum ether (30-60 ℃), shaking for 20s, filtering, repeatedly washing twice, combining filtrates, removing the petroleum ether by rotary evaporation, drying at 105 ℃ to constant weight, and obtaining the mass ratio of the dry weight of the residual solid to the microcapsule product to be detected as the content of the surface pigment, wherein the content is expressed by percentage.
The product accelerated stability evaluation method provided by the invention is a method provided by Chinese pharmacopoeia: and (3) measuring the content of the pigment at different times under the conditions of 40 ℃ and 75% RH to determine the quality of the stability. And the product stability was quickly evaluated as follows: the product stability was expressed as the pigment retention by measuring the pigment content in an open oven at 60 c for the first (0 day), 5 days, 10 days and 20 days. Pigment retention is the ratio of product content to initial content at different times, expressed as a percentage.
Example 1: investigating the influence of the gelatinization process on the formation of starch granules
(1) 500g of corn starch and 500g of maltose are prepared into an aqueous solution with solid content of 45 percent, and after stirring and dispersing at 60 ℃, the temperature is raised to 70 ℃, and stirring is carried out at a constant speed for 30 min. Degassing at-0.07 MPa for 30min, granulating in a starch fluidized bed equipment, wherein the emulsion temperature is 60 deg.C, the air inlet temperature is 100 deg.C, the air inlet temperature of the main tower is 20Hz, the exhaust fan is 45Hz, the atomization pressure is 29Hz, the feed flow rate is 9ml/min, the fluidized bed fan is 20Hz, and the fluidized bed temperature is 50 deg.C to obtain gelatinized starch A with bulk density of 0.35mg/ml, hardness of 15N, and gelatinization strength of 10 Bloom.
(2) Preparing aqueous solution with solid content of 55% from 300g of sodium starch octenyl succinate and 60g of glucose, stirring and dispersing at 60 ℃, heating to 90 ℃, and stirring at constant speed for 15 min. Degassing at-0.1 MPa for 30min, granulating in a starch fluidized bed apparatus in the same manner as in example 1(1), to obtain gelatinized starch B having a bulk density of 0.8mg/ml, a hardness of 105N and a gelatinization strength of 90 Bloom.
(3) 300g of sodium starch octenylsuccinate and 100g of glucose syrup (national label: GB/T20885-. Degassing at-0.1 MPa for 30min, granulating in a starch fluidized bed apparatus in the same manner as in example 1(1), to obtain gelatinized starch C having a bulk density of 0.80mg/ml, a hardness of 135N, and a gelatinization strength of 100 Bloom.
(4) 300g of sodium starch octenylsuccinate and 100g of sucrose are prepared into an aqueous solution with the solid content of 70 percent, and after stirring and dispersing at 60 ℃, the temperature is raised to 90 ℃, and the uniform stirring is carried out for 100 min. Degassing at-0.1 MPa for 30min, granulating in a starch fluidized bed apparatus in the same manner as in example 1(1), to obtain gelatinized starch D having a bulk density of 0.46mg/ml, a hardness of 38N and a gelatinization strength of 50 Bloom.
(5) Comparative example: 300g of pregelatinized corn starch (purchased from Wuhan remote Co-creation science and technology Co., Ltd.) and 100g of glucose syrup are prepared into an aqueous solution with solid content of 60%, and after stirring and dispersing at 60 ℃, the aqueous solution is heated to 90 ℃ and stirred at a constant speed for 60 min. Degassing at-0.1 MPa for 30min, granulating in a starch fluidized bed apparatus in the same manner as in example 1(1), to obtain gelatinized starch E having a bulk density of 0.41mg/ml, a hardness of 32N and a gelatinization strength of 15 Bloom.
(6) Comparative example: 300g of sodium starch octenylsuccinate and 100g of fructo-oligosaccharide (GB/T23528-2009) are prepared into an aqueous solution with 60 percent of solid content, and after stirring and dispersing at 60 ℃, the aqueous solution is heated to 90 ℃ and stirred at a constant speed for 60 min. Degassing at-0.1 MPa for 30min, granulating in a starch fluidized bed apparatus in the same manner as in example 1(1), to obtain gelatinized starch F having a bulk density of 0.38mg/ml, a hardness of 29N and a gelatinization strength of 23 Bloom.
(7) Comparative example: 300G of sodium starch octenylsuccinate and 100G of glucose syrup (national standard: GB/T20885-2007) are prepared into an aqueous solution with 60 percent of solid content, stirred and dispersed at 45 ℃, degassed for 30min under-0.1 MPa, and granulated under starch fluidized bed equipment, the preparation method is the same as that of example 1(1), and the gelatinized starch G is obtained, the bulk density of which is 0.42mg/ml, the hardness of which is 52N and the gelatinization strength of which is 39 Bloom.
As a result, the hardness, bulk density and gel strength of the starch granules after the gelatinization treatment are improved. The starch sodium octenyl succinate and the glucose syrup are gelatinized according to the proportion of 3:1 to obtain the gelatinized starch granules with the strongest hardness, the highest bulk density and the highest gel strength.
Example 2: test of the deoxidizing Effect of ascorbic acid and sodium ascorbate on milk of the present invention
(1) Preparing 300g of sodium starch octenylsuccinate and 100g of fructose into an aqueous solution with solid content of 45%, stirring and dispersing at 60 ℃, heating to 90 ℃, gelatinizing for 30min, and measuring the residual oxygen amount of the emulsion to be 7.2mg/L and the residual oxygen amount to be 7.5mg/L after 24 h. Adding 100g astaxanthin oleoresin (purchased from Daliano biological products Co., Ltd.), homogenizing under 45 + -5 Mpa pressure or dispersing with colloid mill for 30min to obtain emulsion with particle diameter below 1 μm, wet granulating, cutting with cutter at 2000 rpm, stirring at 2500 rpm, granulating for 80s, drying for 30min, and drying at 55 deg.C to obtain astaxanthin microparticle preparation 1, wherein the pigment retention rates are 70.1%, 62.1% and 43.6% respectively at 60 deg.C, open storage for 5 days, and 10 days and 20 days.
(2) Preparing aqueous solution with solid content of 70% from 300g of starch sodium octenylsuccinate and 75g of xylose (GB/T23532-2009), stirring and dispersing at 60 ℃, heating to 90 ℃, and gelatinizing for 30 min. Introducing nitrogen into the emulsion at a flow rate of 0.1ml/min, continuously introducing nitrogen for 30min, and measuring the residual oxygen content of the emulsion to be 0.3mg/L and the residual oxygen content to be 6.5mg/L after 24 h. Adding 100g astaxanthin oleoresin, homogenizing under high pressure of 45 + -5 Mpa or dispersing with colloid mill for 30min to obtain emulsion with particle diameter below 1 μm, and wet granulating to obtain astaxanthin microparticle preparation 2, wherein the pigment retention rates of the preparation are 77.1%, 69.1% and 60.6% at 60 deg.C, and open storage for 5 days, 10 days and 20 days.
(3) Preparing 300g of sodium starch octenylsuccinate and 60g of maltose into an aqueous solution with solid content of 45%, stirring and dispersing at 60 ℃, heating to 90 ℃, and gelatinizing for 30 min. The emulsion is vacuumized under-0.09 MPa, the residual oxygen content of the emulsion is 3.4mg/L, and the residual oxygen content is 6.7mg/L after 24 hours. Adding 100g astaxanthin oleoresin, homogenizing under high pressure of 45 + -5 Mpa or dispersing with colloid mill for 30min to obtain emulsion with particle diameter below 1 μm, and wet granulating to obtain astaxanthin microparticle preparation 3, wherein the pigment retention rates are 73.4%, 65.5% and 55.3% respectively at 60 deg.C and 5 days in open air and 10 days and 20 days.
(4) Preparing aqueous solution with solid content of 70% from 300g of starch sodium octenylsuccinate and 75g of xylose (GB/T23532-2009), stirring and dispersing at 60 ℃, heating to 90 ℃, and gelatinizing for 30 min. The pH value is adjusted to 3.0 by using anhydrous citric acid and 0.1M sodium hydroxide, 1.25g of ascorbic acid and 6.25g of sodium ascorbate are added, the residual oxygen content of the emulsion is measured to be 0.2mg/L, and the residual oxygen content is measured to be 0.2mg/L after 24 hours. Adding 100g astaxanthin oleoresin, homogenizing under high pressure of 45 + -5 Mpa or dispersing with colloid mill for 30min to obtain emulsion with particle diameter below 1 μm, and wet granulating to obtain astaxanthin microparticle preparation 4 with pigment retention rates of 94.1%, 94.7% and 94.2% at 60 deg.C and open air for 5 days, 10 days and 20 days.
(5) 200g of sodium starch octenylsuccinate and 50g of glucose syrup are prepared into an aqueous solution with the solid content of 53 percent, and after stirring and dispersing at 60 ℃, the temperature is raised to 90 ℃ and the gelation is carried out for 30 min. Adjusting pH to 4.5 with anhydrous citric acid and 0.1M sodium hydroxide, adding ascorbic acid 3g and sodium ascorbate 12g, and determining emulsion residual oxygen amount to be 0.1mg/L and residual oxygen amount to be 0.0mg/L after 24 hr. Adding 100g astaxanthin oleoresin, homogenizing under high pressure of 45 + -5 Mpa or dispersing with colloid mill for 30min to obtain emulsion with particle diameter below 1 μm, and wet granulating to obtain astaxanthin microparticle preparation 5 with pigment retention rates of 99.8%, 98.9% and 99.0% at 60 deg.C and open air for 5 days, 10 days and 20 days.
(6) 500g of sodium starch octenylsuccinate and 167g of solid fructose (GB/T26762-2011) are prepared into an aqueous solution with 62 percent of solid content, stirred and dispersed at 60 ℃, heated to 90 ℃ and gelatinized for 30 min. The pH was adjusted to 3.5 with anhydrous citric acid and 0.1M sodium hydroxide, 10.0g of ascorbic acid and 10.0g of sodium ascorbate were added, and the residual oxygen content of the emulsion was determined to be 0.1mg/L and 0.1mg/L after 24 h. Adding 100g astaxanthin oleoresin, homogenizing under high pressure of 45 + -5 Mpa or dispersing with colloid mill for 30min to obtain emulsion with particle diameter below 1 μm, and wet granulating to obtain astaxanthin microparticle preparation 6, which is placed in open air at 60 deg.C for 5 days, and has pigment retention rates of 92.1%, 91.7% and 91.0% in 10 days and 20 days.
As can be seen from the above, ascorbic acid and sodium ascorbate were used in combination in a mass ratio of 1:4 at a pH of 3.5 to 4.5, which is the most effective for deoxygenation of the emulsion of the present invention and the best stability of the obtained product. Although evacuation or introduction of nitrogen also has some effect, the oxygen content of the emulsion rises after standing for a long time, which is disadvantageous in the case of workshop production. The combined use of ascorbic acid and sodium ascorbate can maintain low oxygen content in the emulsion and prevent oxygen from reentering the emulsion, so that the production process is controlled more effectively.
Example 3: preparation and characterization of xanthophyll granule formulation
(1) Preparing aqueous solution with solid content of 60% from 175.5g of sodium starch octenylsuccinate and 58.5g of glucose, stirring and dispersing at 60 ℃, heating to 90 ℃, and gelatinizing for 30 min. Adding 20g of mixed tocopherol, 4g of ascorbyl palmitate and 34g of lutein crystals, grinding by a colloid mill, evaporating and degassing by a thin film, adjusting the pH to 3.0 by using citric acid and sodium hydroxide, adding 20g of ascorbic acid and 20g of sodium ascorbate, granulating by using a starch fluidized bed device, wherein the emulsion temperature is 65 ℃, the air inlet temperature is 100 ℃, the air inlet temperature of a main tower is 20Hz, an exhaust fan is 45Hz, the atomization pressure is 29Hz, the feeding flow rate is 9ml/min, the fluidized bed fan is 20Hz, the fluidized bed temperature is 50 ℃, and the lutein particles A are obtained, the content is 5.95%, the bulk density is 0.7mg/ml, the surface pigment content is 0.03%, and the pigment content is 5.94% when the lutein particles are stored for 6 months at 40 ℃ and 75% RH.
(2) 43.5g of sodium starch octenylsuccinate and 87g of glucose syrup are prepared into an aqueous solution with the solid content of 60 percent, and after stirring and dispersing at 60 ℃, the temperature is raised to 85 ℃ to gelatinize for 30 min. Adding 40g of dl-alpha-tocopherol, 10g of ascorbyl palmitate, 10g of BHT10g and 150g of lutein crystals, grinding by a colloid mill and degassing in vacuum, adjusting the pH to 3.5 by using citric acid and sodium hydroxide, adding 12g of ascorbic acid and 48g of sodium ascorbate, and performing spray condensation granulation, wherein the emulsion temperature is 60 ℃, the air inlet temperature is 80 ℃, the air inlet temperature of a main tower is 25Hz, an exhaust fan is 37Hz, the atomization pressure is 29Hz, the feeding flow rate is 12ml/min, a fluidized bed fan is 20Hz, the fluidized bed temperature is-15 ℃, so that lutein particles B are obtained, the content of the lutein particles B is 10.5%, the bulk density of the lutein particles is 0.75mg/ml, the surface pigment content is 0.05%, and the pigment content is 10.6% when the lutein particles are stored for 6 months under the conditions of 40 ℃ and 75% RH.
(3) Preparing 43.5g of hydroxypropyl distarch phosphate and 87g of glucose syrup into an aqueous solution with solid content of 60%, stirring and dispersing at 60 ℃, heating to 85 ℃, and gelatinizing for 30 min. Adding 40g of dl-alpha-tocopherol, 10g of ascorbyl palmitate, 10g of BHT10g and 150g of lutein crystals, grinding by a colloid mill and degassing in vacuum, adjusting the pH to 3.5 by using citric acid and sodium hydroxide, adding 12g of ascorbic acid and 48g of sodium ascorbate, and performing spray drying granulation, wherein the emulsion temperature is 60 ℃, the air inlet temperature is 160 ℃, the air inlet temperature of a main tower is 20Hz, an exhaust fan is 47Hz, the atomization pressure is 0.3MPa, the feed flow rate is 9ml/min, the air outlet temperature is 80 ℃, and the lutein particles C are obtained, the content is 10.9%, the bulk density is 0.37mg/ml, the surface pigment content is 4.95%, and the pigment content is 4.04% when the lutein particles are stored for 6 months at 40 ℃ and 75% RH.
Example 4: preparation and characterization of beta-carotene microparticle formulations
273g of sodium starch octenyl succinate and 68.25g of sucrose are prepared into an aqueous solution with the solid content of 55%, and the aqueous solution is stirred and dispersed at 60 ℃, heated to 80 ℃ and gelatinized for 15 min. Adding 9g of mixed tocopherol, 4g of ascorbyl palmitate and 110g of beta-carotene crystals, grinding by a colloid mill, degassing in vacuum, adjusting the pH to 4.0 by using citric acid and sodium hydroxide, adding 5.8g of ascorbic acid and 29.2g of sodium ascorbate, granulating under starch fluidized bed equipment, wherein the emulsion temperature is 63 ℃, the air inlet temperature is 60 ℃, the air inlet temperature of a main tower is 18Hz, an exhaust fan is 37Hz, the atomization pressure is 27Hz, the feeding flow rate is 9ml/min, the fluidized bed fan is 20Hz, the fluidized bed temperature is 45 ℃, and the beta-carotene particles D are obtained, the content of the beta-carotene particles D is 21.34%, the bulk density of the beta-carotene particles D is 0.45mg/ml, the surface pigment content of the beta-carotene particles D is 1.74%, and the pigment content of the beta-carotene particles D is 10.19% when the beta-carotene particles are stored for 6 months under the conditions of 40 ℃ and 75% RH.
Example 5: preparation and characterization of zeaxanthin microparticle formulations
(1) 226g of starch sodium octenylsuccinate and 45.2g of fructo-oligosaccharide (GB/T23528-2009) are prepared into an aqueous solution with solid content of 63%, stirred at 60 ℃ and dispersed, heated to 75 ℃ and gelatinized for 60 min. BHT2g, 8g of alpha-tocopherol, 34g of zeaxanthin crystals were added, colloid-milled and film-falling degassed, the pH was adjusted to 4.0 with citric acid and sodium hydroxide, and then 2g of ascorbic acid, 6g of sodium ascorbate were added, and spray-dried and granulated to obtain zeaxanthin fine particles E having a content of 5.53%, a bulk density of 0.49mg/ml, a surface pigment content of 0.53%, and a pigment content of 2.26% when stored at 40 ℃, 75% RH for 6 months.
(2) 226g of sodium starch octenylsuccinate and 45.2g of glucose are prepared into an aqueous solution with solid content of 63 percent, and after stirring and dispersing at 60 ℃, the temperature is raised to 75 ℃ to gelatinize for 60 min. Adding BHT2g, alpha-tocopherol 8g, zeaxanthin crystals 34g, shearing, emulsifying and vacuum degassing, adjusting pH to 4.0 with citric acid and sodium hydroxide, adding ascorbic acid 2g and sodium ascorbate 6g, spray drying and granulating to obtain zeaxanthin fine particles F with content of 5.43%, bulk density of 0.77mg/ml, surface pigment content of 0.01%, and pigment content of 5.49% when stored at 40 deg.C and 75% RH for 6 months.
Example 6: preparation and characterization of astaxanthin microparticle formulations
254.4g of sodium starch octenylsuccinate and 63.6g of isomaltooligosaccharide are prepared into an aqueous solution with the solid content of 70%, stirred and dispersed at 45 ℃, heated to 75 ℃ and gelatinized for 100 min. 12G of propyl gallic acid and 126G of astaxanthin oleoresin, shearing, emulsifying, vacuum degassing, adjusting the pH value to 4.5 by using citric acid and sodium hydroxide, adding 6G of ascorbic acid and 24G of sodium ascorbate, and performing spray condensation granulation to obtain astaxanthin fine particles G with the content of 2.12 percent, the bulk density of 0.38mg/ml, the surface pigment content of 3.51 percent and the pigment content of 0.50 percent when the astaxanthin fine particles are stored for 6 months at 40 ℃ and 75 percent RH.
Example 7: preparation and characterization of lycopene microparticle formulations
155.1g of sodium starch octenylsuccinate and 30.6g of maltose are prepared into an aqueous solution with the solid content of 60 percent, and after stirring and dispersing at 60 ℃, the temperature is raised to 80 ℃ to gelatinize for 50 min. Adding 6.6g of mixed tocopherol, 2.4g of ascorbyl stearate and 40.8g of lycopene crystals, grinding by a colloid mill and degassing, adjusting the pH to 5.0 by using citric acid and sodium hydroxide, adding 0.75g of ascorbic acid and 2.25g of sodium ascorbate, granulating by a dry granulator at the air inlet temperature of 150 ℃ and the air exhaust temperature of 100 ℃ to obtain lycopene particles H with the content of 10.88 percent, the bulk density of 0.66mg/ml, the surface pigment content of 0.2 percent and the pigment content of 3.81 percent when the lycopene particles are stored for 6 months at 40 ℃ and 75 percent RH.
Example 8: preparation and characterization of lutein ester microparticle formulations
85.2g of sodium starch octenylsuccinate and 21.4g of glucose syrup are prepared into an aqueous solution with the solid content of 55 percent, and after stirring and dispersing at 60 ℃, the temperature is raised to 90 ℃ and gelatinization is carried out for 30 min. 2.0g of t-butylhydroxyquinoline, 6.0g of mixed tocopherol and 29.4g of lutein ester crystals were added, homogenized under high pressure and degassed, the pH was adjusted to 6.0 with citric acid and sodium hydroxide, and then 2g of ascorbic acid and 10g of sodium ascorbate were added, and granulated under a starch fluidized bed apparatus to obtain lutein ester fine particles I having a content of 11.02%, a bulk density of 0.68mg/ml, a surface pigment content of 0.3%, and a pigment content of 10.99% when stored at 40 ℃ and 75% RH for 6 months.
Example 9: carotenoid product tabletting stability test
The carotenoid fine particles of examples 3-8 and multivitamin tabletting excipients were mixed and then tabletted using a Tianfeng ZPW-8 rotary tablet press to obtain a composite carotenoid vitamin tablet with a tablet hardness of 80-100N and a friability of 0.5% or less, which was packaged in an HDPE bottle sealed with a lid with a heat-sealed aluminum foil, and stored at 40 ℃ and 75% relative humidity for 6 months, with the product content and stability shown in Table 1.
TABLE 1
Figure BDA0001529331430000101

Claims (5)

1. The carotenoid particle preparation is prepared by emulsifying a raw material mixture containing carotenoid and a gelation wall material and granulating; the method is characterized in that the gelatinized wall material is obtained by gelatinizing a wall material mixture of starch and carbohydrate according to a mass ratio of 3: 1; wherein the starch is sodium starch octenyl succinate; the carbohydrate is glucose and/or glucose syrup; the gelation treatment is to prepare the wall material mixture into aqueous solution with solid content of 45-70%, stir at 60 ℃ for dispersion and dissolution for 30min, and then stir at 80-90 ℃ for 15-100 min; the raw material mixture is emulsified and then added with a deoxidizer to remove oxygen in the emulsion, wherein the deoxidizer is a mixture of ascorbic acid and sodium ascorbate according to a mass ratio of 1: 1-5; the dosage of the deoxidizer is 1-10% of the mass of the carotenoid microparticle preparation.
2. The carotenoid microparticle formulation as claimed in claim 1, wherein the amount of the gelling wall material is 30-65% by mass of the carotenoid microparticle formulation.
3. The carotenoid microparticle formulation as claimed in claim 1, wherein the raw material mixture further contains an antioxidant selected from tocopherol, fatty acid ascorbate, butylhydroxytoluene, butylhydroxyanisole, propyl gallic acid, t-butylhydroxyquinoline or a mixture thereof; the dosage of the antioxidant is 0.1-10% of the mass of the carotenoid microparticle preparation.
4. The carotenoid microparticle formulation as defined in claim 1, wherein said carotenoid is selected from the group consisting of lutein, zeaxanthin, lycopene, α -carotene, β -carotene, canthaxanthin, lutein esters, astaxanthin, and mixtures thereof.
5. A process for preparing a carotenoid microparticle formulation as defined in claim 1, comprising the steps of: a) preparing the raw material mixture into emulsion with the particle size of 0.5-1 mu m; b) adding a deoxidizing agent to remove oxygen in the emulsion; c) granulating to obtain carotenoid microparticle preparation.
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